CN108690983B - Wear-resistant corrosion-resistant Cr/CrAlSiN composite coating, and preparation method and application thereof - Google Patents
Wear-resistant corrosion-resistant Cr/CrAlSiN composite coating, and preparation method and application thereof Download PDFInfo
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
- C23C28/322—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer only coatings of metal elements only
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
- C23C14/0084—Producing gradient compositions
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
- C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/36—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases using ionised gases, e.g. ionitriding
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D2201/00—Treatment for obtaining particular effects
- C21D2201/03—Amorphous or microcrystalline structure
Abstract
The invention discloses a wear-resistant corrosion-resistant Cr/CrAlSiN composite coating, which comprises a bonding layer and a wear-resistant corrosion-resistant layer which are sequentially formed on a substrate, wherein the bonding layer adopts a Cr layer, the wear-resistant corrosion-resistant layer adopts a CrAlSiN layer, and the CrAlSiN layer has an amorphous nanocrystalline structure and comprises a face-centered cubic CrN phase, an AlN reinforcing phase and an amorphous Si phase3N4Phase of the amorphous Si3N4And the CrN phase and the AlN strengthening phase are coated. The composite coating has excellent bearing wear resistance and corrosion resistance, can meet the high-performance requirements on various parts and facilities under severe working conditions, and has good application prospect. The invention also discloses a preparation method of the composite coating, which is simple and feasible and can realize batch production.
Description
Technical Field
The invention relates to a wear-resistant corrosion-resistant coating, in particular to a wear-resistant corrosion-resistant Cr/CrAlSiN composite coating and a preparation method thereof, which are applied to marine environments such as marine equipment, offshore facilities, ships and naval vessels, and belong to the technical field of material corrosion.
Background
With the gradual development and utilization of deep sea resources, ocean engineering materials face huge corrosion and abrasion, the problem seriously restricts the development of important ocean engineering technologies and equipment, the corrosion failure problem seriously influences the reliability and the service life of the ocean engineering and the equipment, and the corrosion protection technology of the materials becomes a problem to be solved urgently in the ocean engineering field of China. For example, valves, sealing rings and the like which are used as key friction parts in direct contact with seawater are in seawater medium for a long time and are seriously corroded and abraded in the using process, and the service conditions are quite harsh. The physical vapor deposition technology (PVD method) is used for depositing a protective coating from nanometer to micron on the surface of a workpiece, the thickness of the coating is accurate and controllable, the use size of a precise part is not influenced, and an effective protection method is provided for solving the problem of a key friction part in service under a severe condition.
Until now, CrN coatings have been widely used in various industries due to their advantages of high hardness, good wear resistance, stable chemical properties, etc., and have become one of the PVD protective coatings with the widest application and the most stable performance. However, conventional CrN coatings tend to form penetrating corrosion channels in corrosive media due to their remarkable columnar crystal structure, which in turn leads to material peeling and even failure, especially under high load conditions. Therefore, the traditional CrN coating can not meet the workpiece requirements in the extreme ocean environment.
Disclosure of Invention
The invention mainly aims to provide a wear-resistant corrosion-resistant Cr/CrAlSiN composite coating, a preparation method and application thereof, so as to overcome the defects in the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
the embodiment of the invention provides a wear-resistant corrosion-resistant Cr/CrAlSiN composite coating, which comprises a bonding layer and a wear-resistant corrosion-resistant layer, wherein the bonding layer and the wear-resistant corrosion-resistant layer are sequentially formed on a substrate, the bonding layer adopts a Cr layer, and the wear-resistant corrosion-resistant layer adopts a CrAlSiN layer.
Further, the CrAlSiN layer has an amorphous nanocrystalline structure and comprises a CrN phase, an AlN reinforcing phase and amorphous Si in a face-centered cubic structure3N4Phase of the amorphous Si3N4And the CrN phase and the AlN strengthening phase are coated.
Preferably, the CrAlSiN layer contains 10-20 wt% of CrN phase, 6-10 wt% of AlN phase and 6-10 wt% of Si3N4The phase content is 15 to 45 wt%.
The embodiment of the invention also provides a method for preparing the wear-resistant corrosion-resistant Cr/CrAlSiN composite coating, which comprises the following steps:
carrying out ion nitriding treatment and/or ion etching treatment on the surface of the matrix;
and depositing a Cr layer and a CrAlSiN layer on the surface of the matrix in sequence to form the composite coating.
In some preferred embodiments, the preparation method may further comprise: and cleaning the surface of the substrate, and then sequentially performing ion nitriding treatment and ion etching treatment on the clean substrate surface.
The embodiment of the invention also provides application of the wear-resistant corrosion-resistant Cr/CrAlSiN composite coating in the field of surface protection of metal materials and/or non-metal materials. Preferably, the metallic material and/or the non-metallic material comprises a marine engineering material.
Compared with the prior art, the invention has at least the following advantages:
(1) the wear-resistant corrosion-resistant Cr/CrAlSiN composite coating disclosed by the invention adopts the design of the transition layer, so that the binding force between the substrate and the coating is effectively improved, the bearing and wear-resistant capacity of the coating is also greatly improved, and particularly, Si is formed by Si with different contents in the CrAlSiN layer3N4The amorphous structure disturbs the crystal orientation growth of CrN and AlN to make Si3N4The amorphous structure wraps CrN and AlN crystals, so that the failure and peeling of the coating caused by the penetration of a corrosive medium through the coating can be effectively prevented, and the corrosion resistance of the coating is remarkably improved.
(2) The preparation method adopts the multi-arc ion plating technology, can prepare the Cr/CrAlSiN composite coating by controlling the argon flow and the nitrogen flow and changing the Al-Si ratio in the AlSi target, and enables the components of the CrAlSiN layer to be adjustable, so that the composite coating has excellent wear resistance, corrosion resistance and contact fatigue resistance, the preparation process is simple and easy to implement, and batch production can be realized;
(3) the wear-resistant corrosion-resistant Cr/CrAlSiN composite coating can meet the high-performance requirements on parts such as valve sealing elements, gears, fasteners and the like under severe working conditions, and has a good application prospect in high-precision water and gas conveying system equipment, petrochemical engineering pipelines, nuclear power station equipment and the like.
Drawings
FIGS. 1 a-1 f are cross-sectional profiles of some exemplary Cr/CrAlSiN composite coatings in example 1 of the present invention, respectively.
FIG. 2 is an XRD spectrum of some typical Cr/CrAlSiN composite coatings in example 1 of the present invention.
FIG. 3 is an XPS fit spectrum of Si within composite coating numbered S2 in example 1 of the present invention.
FIG. 4 is a graph of the nano-hardness of some typical Cr/CrAlSiN composite coatings in example 1 of the present invention.
FIG. 5 is a polarization curve of some exemplary Cr/CrAlSiN composite coatings in example 1 of the present invention.
FIG. 6 is a graph showing the wear rate of some typical Cr/CrAlSiN composite coatings in the seawater environment in example 1 of the present invention.
Detailed Description
One aspect of the embodiment of the invention provides a wear-resistant corrosion-resistant Cr/CrAlSiN composite coating, which comprises a bonding layer and a wear-resistant corrosion-resistant layer, wherein the bonding layer and the wear-resistant corrosion-resistant layer are sequentially formed on a substrate, the bonding layer adopts a Cr layer, and the wear-resistant corrosion-resistant layer adopts a CrAlSiN layer.
The bonding layer can also be regarded as a bottom layer of the composite coating or a transition layer between the wear-resistant and corrosion-resistant layer and the substrate.
Wherein, the wear-resistant and corrosion-resistant layer can also be used as a surface layer.
Preferably, the thickness of the composite coating is 5 to 20 μm.
Preferably, the thickness of the Cr layer is 0.2 to 1 μm.
Preferably, the CrAlSiN layer has a thickness of 4.8 to 19 μm.
Preferably, the Si content of the craalsin layer is 2at.% to 10 at.%.
Preferably, the content of Al and Si in the AlSi target material is 9: 1-1: 1;
preferably, the CrAlSiN layer has an amorphous nanocrystalline structure and includes a face-centered cubic CrN phase, an AlN reinforcing phase and amorphous Si3N4Phase of the amorphous Si3N4And the CrN phase and the AlN strengthening phase are coated.
Preferably, the CrAlSiN layer contains 10-20 wt% of CrN phase, 6-10 wt% of AlN phase and 6-10 wt% of Si3N4The phase content is 15 to 45 wt%.
The substrate may be selected from metal substrates, and may be a hard alloy such as stainless steel.
Further, the composite coating is directly formed on the surface of the substrate, and the surface of the substrate is subjected to ion nitriding treatment in advance. More preferably, the surface of the substrate is also subjected to an ion etching treatment in advance to remove surface oxidation substances and contaminants.
The preparation method of the wear-resistant corrosion-resistant Cr/CrAlSiN composite coating provided by the embodiment of the invention comprises the following steps:
carrying out ion nitriding treatment and/or ion etching treatment on the surface of the matrix;
and depositing a Cr layer and a CrAlSiN layer on the surface of the matrix in sequence to form the composite coating.
In some preferred embodiments, the preparation method comprises: the surface of the substrate is cleaned, and then the clean substrate surface is sequentially subjected to ion nitriding treatment and ion etching treatment, so that the surface cleaning agent has the function of purifying the surface and can remove a passive film and pollutants on the surface of a workpiece.
Further, the surface cleaning process includes: and sequentially carrying out ultrasonic cleaning on the surface of the matrix by using an oil removal agent and more than one organic solvent until the surface of the matrix is clean.
For example, the surface cleaning treatment may specifically include: firstly, a sample (matrix) is put into an oil removing agent (such as petroleum ether) and is cleaned by ultrasonic for more than 30min to remove oil stains on the surface of the sample, then the sample is put into acetone and is cleaned by ultrasonic for 10-20min, then the sample is cleaned by ultrasonic for 10-20min in absolute ethyl alcohol, finally the sample is taken out and is dried by nitrogen, and then ion nitriding treatment is carried out.
In some preferred embodiments, the ion nitriding treatment comprises: putting a substrate with a clean surface into a cavity of coating equipment, introducing nitrogen, controlling the working pressure to be 8-10 Pa, applying negative bias of-800-1000V on the substrate, controlling the temperature to be 450-500 ℃, and nitriding for 2-4 h.
Preferably, in the ion nitriding treatment process, the flow rate of the nitrogen is 1000-1200 sccm.
Preferably, the purity of the nitrogen gas is above 99.95% during the ion nitriding treatment.
In some preferred embodiments, the ion etching process comprises placing the substrate into a chamber of a coating apparatus and evacuating the chamber to a vacuum of 3 × 10-3Pa～5×10-3Pa, heating the substrate to 400-450 ℃, and then etching the substrate surface applied with negative bias by utilizing Ar plasma.
Further preferably, the ion etching treatment conditions include: the flow of the high-purity Ar is controlled to be 100-300sccm, a Cr target is selected as a direct current power supply, the target current is set to be 50-70A, and the surface of the substrate is continuously bombarded under the bias voltage of-900V to-1200V for 5-10 min.
Preferably, during the ion etching treatment, the purity of the high-purity argon gas is more than 99%.
Preferably, the purity of the Cr target is more than 99% in the ion etching treatment process.
In some preferred embodiments, the preparation method specifically comprises: placing the substrate subjected to ion nitriding treatment and/or ion etching treatment in a cavity of coating equipment, selecting a Cr target, setting the target current to be 40-100A, applying negative bias of-20-50V on the substrate, controlling the heating temperature to be 400-450 ℃, keeping the argon flow to be 300-350 sccm, and depositing for 0.5-1 h, thereby depositing the Cr layer on the surface of the substrate.
Preferably, the purity of the argon gas is more than 99%.
Preferably, the purity of the Cr target is more than 99%.
In some preferred embodiments, the preparation method specifically comprises: placing the substrate with the Cr layer deposited on the surface in a cavity of a coating device, selecting Cr and AlSi targets, setting the target current to be 40-100A, applying negative bias of-20-50V on the substrate, controlling the heating temperature to be 400-450 ℃, keeping the argon flow to be 0-100 sccm, controlling the nitrogen flow to be 500-700 sccm, and depositing for 2-4 h, thereby forming the CrAlSiN coating in a deposition manner.
Preferably, the Si content of the craalsin layer can be adjusted within the range of 0, 2at.% to 10at.% by controlling the ratio of Al to Si in the AlSi target.
Preferably, the purity of both the Cr target and the AlSi target is 99.9% or more.
Preferably, the purity of the nitrogen is more than 99.9%.
Preferably, a plurality of sets of targets are arranged in the coating equipment, each set of targets comprises more than one Cr target and more than one AlSi target, and one Cr target in each set of targets and a corresponding AlSi target are arranged perpendicularly to each other.
In some preferred embodiments, the preparation method may further comprise: sequentially performing ion nitriding treatment and ion etching treatment on the surface of a substrate in a cavity of coating equipment, sequentially depositing a Cr layer and a CrAlSiN layer on the surface of the substrate, cooling the obtained composite coating to below 220 ℃ in a vacuum environment, and cooling to below 100 ℃ in a protective atmosphere.
In some more specific embodiments of the present invention, a method for preparing the Cr/craalsin composite coating may comprise the steps of:
(1) sample pretreatment: the surface of the sample (i.e., the substrate) is subjected to cleaning treatment in the manner described above, followed by ion nitriding treatment;
preferably, the ion nitriding treatment is specifically: and (3) placing the cleaned substrate in a cavity of coating equipment, introducing nitrogen gas with the flow rate of 1000-1200 sccm, controlling the working pressure at 8-10 Pa, applying negative bias of-800-1000V to the substrate, controlling the temperature at 450-500 ℃, and nitriding for 2-4 h.
(2) Ion etching, namely placing a sample in a cavity of coating equipment, and vacuumizing the back to (3-5) × 10-3Pa, heating the substrate to 400-450 ℃, and then bombarding and activating the surface of the substrate applied with negative bias by using argon plasma. Preferably, high-purity Ar can be introduced, the flow rate is controlled at 100-300sccm, a Cr target is selected as a direct current power supply, the target current is set to be 50-70A, and the sample is continuously bombarded under the bias voltage of-900V to-1200V for 5-10 min.
(3) Depositing a transition layer: in order to improve the binding force of the coating, a Cr target is selected, the target current is set to be 40-100A, negative bias of-20 to-50V is applied to a workpiece, the heating temperature is controlled to be 400-450 ℃, the argon flow is kept to be 300-350 sccm, and the deposition time is 0.5-1 h, so that the Cr transition layer is obtained.
(4) Deposition of a CrAlSiN coating: selecting Cr and AlSi targets, setting target current to be 40-100A, applying negative bias voltage of-20 to-50V on a workpiece, controlling the heating temperature to be 400-450 ℃, keeping argon flow to be 0-100 sccm, controlling nitrogen flow to be 500-700 sccm, and depositing for 2-4 h, and obtaining CrAlSiN layers with different Si contents (for example, Si contents are 0, 2at.%, 4 at.%, 6 at.%, 8 at.% or 10 at.%) by controlling the proportion of Al and Si in the AlSi targets, wherein the wear resistance and corrosion resistance of the coating can be improved by changing the Si content.
(5) Taking out a sample: after the deposition of the composite coating is finished, cooling to below 220 ℃ in a vacuum environment, then cooling to below 100 ℃ in a nitrogen protective atmosphere, finally discharging to atmospheric pressure, opening a cavity and discharging, and thus obtaining the composite coating on the surface of the substrate.
The invention also provides application of the wear-resistant corrosion-resistant Cr/CrAlSiN composite coating in the field of surface protection of metal materials and/or non-metal materials.
Preferably, the metallic material and/or the non-metallic material comprises a marine engineering material.
For example, the embodiment of the invention also provides equipment, and the wear-resistant corrosion-resistant Cr/CrAlSiN composite coating is coated on at least partial area on the surface and/or inside the equipment. The equipment may be, but is not limited to, high precision water and gas transport system equipment, petrochemical pipelines, nuclear power plant equipment, and the like.
For example, the embodiment of the invention also provides a type of marine rapid development equipment, and at least a local area on the surface and/or inside of the marine rapid development equipment is covered with the wear-resistant and corrosion-resistant Cr/CrAlSiN composite coating.
For example, the embodiment of the invention also provides a workpiece, and the wear-resistant corrosion-resistant Cr/CrAlSiN composite coating is coated on at least partial area of the surface and/or the interior of the workpiece. The composite coating can meet the high-performance requirements on workpieces such as valve sealing elements, gears, fasteners and the like under severe working conditions.
The technical solution of the present invention is further described in detail below with reference to the accompanying drawings and several embodiments.
Example 1: the process for forming the Cr/CrAlSiN composite coating on the surface of the steel ball 304 by taking the steel ball as a sample comprises the following steps:
(1) sample pretreatment: in order to remove oil stains on the surface of a sample, the sample is firstly placed in an oil removing agent (such as petroleum ether) and is subjected to ultrasonic cleaning for 30min, then is placed in acetone and is subjected to ultrasonic cleaning for 10min, then is subjected to ultrasonic cleaning in absolute ethyl alcohol for 10min, and finally is taken out and is dried by blowing with nitrogen gas to perform ion nitriding treatment.
Preferably, the ion nitriding treatment specifically includes: and (3) placing the cleaned substrate in a cavity of coating equipment, introducing nitrogen gas with the flow rate of 1000sccm, controlling the working pressure at 8Pa, applying negative bias of-800V to the substrate, controlling the temperature at 450 ℃, and performing nitriding treatment for 2 h. Wherein the purity of the nitrogen is more than 99.95 percent.
(2) Ion etching, namely putting the sample into a cavity of coating equipment, heating the substrate to 400 ℃, and vacuumizing the cavity to 3 × 10-3And after Pa, bombarding and activating the surface of the substrate applied with negative bias by using argon plasma. Introducing high-purity Ar, controlling the flow at 100sccm, selecting a Cr target as a direct current power supply, setting the target current to be 50A, and continuously bombarding the sample for 8min under the bias voltage of-900V. Preferably, the purity of the argon is more than 99%. Preferably, the purity of the Cr target used is 99% or more.
(3) Depositing a transition layer: in order to improve the binding force of the coating, a Cr target is selected, the target current is set to be 40A, negative bias of-20V is applied to the workpiece, the heating temperature is controlled to be 400 ℃, the argon flow is kept to be 100sccm, and the deposition time is 0.5h, so that the Cr transition layer is obtained. Preferably, the purity of the argon is more than 99%. Preferably, the purity of the Cr target used is 99% or more.
(4) Deposition of a CrAlSiN coating: selecting Cr and AlSi targets, setting the target current to be 40A, applying negative bias voltage of-20V on a workpiece, controlling the heating temperature to be 400 ℃, keeping the argon flow to be 100sccm, controlling the nitrogen flow to be 500sccm, and controlling the deposition time to be 2h, and obtaining CrAlSiN layers with different Si contents by controlling the proportion of Al to Si in the AlSi targets (for example, the Si contents are respectively 0, 2at.%, 4 at.%, 6 at.%, 8 at.%, and 10 at.%), wherein the obtained Cr/CrAlSiN composite coating can be sequentially named as S0, S1, S2, S3, S4, and S5. Preferably, the purity of the argon is more than 99%, and the purity of the nitrogen is more than 99.95%. Preferably, the purity of the Cr and AlSi target is 99% or more. Preferably, the Cr target and the AlSi target in the coating apparatus are arranged in groups, and the Cr target and the AlSi target in each group are arranged vertically.
(5) Taking out a sample: after the deposition of the composite coating is finished, cooling the sample to below 220 ℃ in a vacuum environment in coating equipment, then cooling to below 100 ℃ in a nitrogen protective atmosphere, finally discharging to atmospheric pressure, opening the cavity and discharging, and thus obtaining the composite coating on the surface of the substrate.
The method comprises the steps of using a FEI Quanta FEG 250 field emission scanning electron microscope to represent the cross section morphology of a coating, selecting an ETD detector to perform imaging analysis under the condition that the electron gun acceleration voltage is 8-10 kV, using a Bruker-AXS D8 advanced X-ray diffractometer to scan the coating at the step length of 0.02 DEG under the conditions of 40mA and 40kV, and using a Kratos-Axis Ultra D L D X-ray photoelectron spectrometer (XPS) to perform element valence and chemical bond composition analysis on the coating, wherein the experimental result shows that the CrN coating presents an obvious columnar crystal structure and the lowest thickness, the CrAlSiN coating is compact in structure, and the coating thickness presents an increasing trend along with the increase of silicon content (shown in figures 1 a-1 f, which respectively correspond to S0, S1, S2, S3, S4 and S5), the XRD map shown in figure 2 and the map shown in figure 3, the CrN coating mainly comprises a face-phase cubic structure, and amorphous Si and Al and AlN phase strengthening are generated in the coating after doping3N4Phase, forming a typical amorphous nanocrystalline structure, improving the coating properties, and Si3N4The phase can react with water to form silica gel (Si (OH) during friction4) Has good lubricating effect.
On a PGSTAT302 type Autolab electrochemical workstation, a saturated calomel electrode is selected as a reference electrode, a platinum electrode is selected as an auxiliary electrode, and the composite coatings of S0, S1, S2, S3, S4 and S5 are selected as working electrodes to jointly form three electrode systems, and Tafel curve measurement is carried out in an artificial standard seawater environment; the hardness and the elastic modulus of the coating are measured by a continuous rigidity method by selecting an MTS-Nano G200 nanometer press-in test platform, 6 different areas are selected on a sample, the sample is pressed into a fixed depth (1000nm) by a Berkovich diamond pressure head and then unloaded to obtain a press-in-unloading curve, the hardness of the coating is obtained by calculation, and then an average value is taken.
The friction and wear life of the composite coatings of S0, S1, S2, S3, S4 and S5 in a seawater environment is evaluated by a UMT-3 multifunctional friction and wear testing machine, and a reciprocating sliding mode is adopted in a friction experiment, the sliding frequency is 5Hz, the load is 10N, the ambient temperature is 20 ℃, the relative humidity is 70%, and phi is 3mm YG-6 hard WC alloy balls as a friction pair. The test result shows that: the hardness of the CrN coating is about 19GPa, and after Al and Si are doped, the hardness of the coating is obviously improved and reaches the highest value of 38GPa when the silicon content is 4at percent (S2); meanwhile, the corrosion current density of the CrN coating is in the E-6 th power, and after Al and Si are doped, the corrosion current density of the coating is reduced by one order of magnitude (E-7 th power), so that the corrosion resistance is obviously improved; in a seawater environment, the wear rate of the CrN coating reaches the highest, after Al and Si are doped, the wear rate of the coating is reduced by 1-2 orders of magnitude, wherein the wear rate reaches the lowest when the Si content is 4 at% (S2), and the best wear resistance is shown.
Example 2: the process for forming the Cr/CrAlSiN composite coating on the surface of the ball valve made of 316 stainless steel as a substrate comprises the following steps:
(1) sample pretreatment: in order to remove oil stains on the surface of a sample, the sample is firstly placed in an oil removing agent (such as petroleum ether) and is subjected to ultrasonic cleaning for 30min, then is placed in acetone and is subjected to ultrasonic cleaning for 10min, then is subjected to ultrasonic cleaning in absolute ethyl alcohol for 10min, and finally is taken out and is dried by blowing with nitrogen gas to perform ion nitriding treatment.
Preferably, the ion nitriding treatment is specifically: and (3) placing the cleaned substrate in a vacuum cavity of coating equipment, introducing nitrogen gas with the flow rate of 1200sccm, controlling the working pressure at 9Pa, applying negative bias of-1000V to the substrate, controlling the temperature at 500 ℃, and performing nitriding treatment for 4 hours. Preferably, the purity of the nitrogen gas is 99.95% or more.
(2) Ion etching: placing the sample in a vacuum cavity of a coating device, heating the matrix to 450 ℃, and vacuumizing the cavityPre-pumping to 5 × 10-3And after Pa, bombarding and activating the surface of the substrate applied with negative bias by using argon plasma. Introducing high-purity Ar, controlling the flow at 300sccm, selecting a Cr target as a direct-current power supply, setting the target current to be 70A, and continuously bombarding the sample for 8min under the bias of-1200V. Preferably, the purity of the argon is more than 99%. Preferably, the purity of the Cr target used is 99% or more.
(3) Depositing a transition layer: in order to improve the binding force of the coating, a Cr target is selected, the target current is set to be 100A, negative bias of-50V is applied to the workpiece, the heating temperature is controlled to be 450 ℃, the argon flow is kept to be 300sccm, and the deposition time is 1h, so that the Cr transition layer is obtained. Preferably, the purity of the argon is more than 99%. Preferably, the purity of the Cr target used is 99% or more.
(4) Deposition of CrAlSiN coating
Selecting Cr and AlSi targets, setting the target current as 100A, applying minus 50V bias on a workpiece, controlling the heating temperature to be 450 ℃, keeping the argon flow at 0sccm, controlling the nitrogen flow at 600sccm, and controlling the deposition time to be 2h, so as to obtain CrAlSiN layers (0, 2at.%, 4 at.%, 6 at.%, 8 at.%, 10 at.%) with different Si contents by controlling the ratio of Al to Si in the AlSi targets. Preferably, the purity of the argon is more than 99%, and the purity of the nitrogen is more than 99.95%. Preferably, the purity of the Cr and AlSi target is 99% or more.
Example 3: a butterfly valve made of 316 stainless steel is used as a base body, and the method comprises the following steps: the process for forming the Cr/CrAlSiN composite coating on the surface of the Cr/CrAlSiN composite coating comprises the following steps:
(1) sample pretreatment: in order to remove oil stains on the surface of a sample, the sample is firstly placed in an oil removing agent (such as petroleum ether) and is subjected to ultrasonic cleaning for 30min, then is placed in acetone and is subjected to ultrasonic cleaning for 15min, then is subjected to ultrasonic cleaning for 15min in absolute ethyl alcohol, and finally is taken out and is dried by blowing with nitrogen gas to perform ion nitriding treatment.
Preferably, the ion nitriding treatment is specifically: and (3) placing the cleaned substrate in a vacuum cavity of coating equipment, introducing nitrogen gas with the flow rate of 1100sccm, controlling the working pressure at 9Pa, applying negative bias of-900V to the substrate, controlling the temperature at 480 ℃, and performing nitriding treatment for 3 hours. Preferably, the purity of the nitrogen gas is 99.95% or more.
(2) Ion etching, namely placing the sample in a vacuum cavity of coating equipment, heating the substrate to 430 ℃, and vacuumizing the cavity to 4 × 10-3And after Pa, bombarding and activating the surface of the substrate applied with negative bias by using argon plasma. Introducing high-purity Ar, controlling the flow at 200sccm, selecting a Cr target as a direct-current power supply, setting the target current to be 60A, and continuously bombarding the sample for 8min under the bias of-1100V. Preferably, the purity of the argon is more than 99%. Preferably, the purity of the Cr target used is 99% or more.
(3) Depositing a transition layer: in order to improve the binding force of the coating, a Cr target is selected, the target current is set to be 70A, negative bias of-35V is applied to the workpiece, the heating temperature is controlled to be 430 ℃, the argon flow is kept to be 325sccm, and the deposition time is 0.75h, so that the Cr transition layer is obtained. Preferably, the purity of the argon is more than 99%. Preferably, the purity of the Cr target used is 99% or more.
(4) Deposition of CrAlSiN coating
Selecting Cr and AlSi targets, setting the target current to be 70A, applying negative bias voltage of-35V on a workpiece, controlling the heating temperature to be 430 ℃, keeping the argon flow to be 50sccm, controlling the nitrogen flow to be 550sccm, and controlling the deposition time to be 3h, thereby obtaining CrAlSiN layers (0, 2at.%, 4 at.%, 6 at.%, 8 at.%, 10 at.%) with different Si contents by controlling the ratio of Al to Si in the AlSi targets. Preferably, the purity of the argon is more than 99%, and the purity of the nitrogen is more than 99.95%. Preferably, the purity of the Cr and AlSi target is 99% or more.
Similar test results to those of example 1 can also be obtained by testing the morphology, structure and performance of a series of Cr/CrAlSiN composite coatings obtained in examples 2 and 3 in a manner similar to that of example 1.
In addition, the inventor also refers to the schemes of examples 1-3 and carries out a series of experiments by adopting other process conditions recorded in the specification, and prepares a series of Cr/CrAlSiN composite coatings, and tests show that the Cr/CrAlSiN composite coatings have excellent wear resistance, corrosion resistance and contact fatigue resistance.
Therefore, the Cr/CrAlSiN composite coating can effectively protect the matrix, so that the matrix meets the high-performance requirement under the severe working condition, the service life is prolonged, and the long-term stable operation of equipment is ensured. The Cr/CrAlSiN composite coating is particularly suitable for being used as an appearance coating of mechanical motion basic parts such as various valves, gears, fasteners and the like in a seawater environment.
It should be understood that the above-mentioned embodiments are illustrative of the preferred embodiments of the present invention, but the present invention is not limited to the above-mentioned embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and they are included in the scope of the present invention.
Claims (14)
1. A preparation method of a wear-resistant corrosion-resistant Cr/CrAlSiN composite coating is characterized by comprising the following steps:
performing ion nitriding treatment and/or ion etching treatment on the surface of a substrate, wherein the ion nitriding treatment comprises the steps of placing the substrate with a clean surface into a cavity of coating equipment, introducing nitrogen, controlling the flow of the nitrogen to be 1000-1200 sccm, controlling the working pressure to be 8-10 Pa, applying negative bias of-800-1000V to the substrate, controlling the temperature to be 450-500 ℃, and performing nitriding treatment for 2-4 h, and the ion etching treatment comprises the steps of placing the substrate into the cavity of the coating equipment, and vacuumizing the cavity to be 3 × 10-3Pa～5×10-3Pa, heating the substrate to 400-450 ℃, and etching the surface of the substrate applied with negative bias by using Ar plasma, wherein the ion etching treatment conditions comprise: controlling the flow of high-purity Ar to be 100-300sccm, selecting a Cr target as a direct current power supply, setting the target current to be 50-70A, and continuously bombarding the surface of the substrate for 5-10 min under the bias voltage of-900 to-1200V;
placing the substrate subjected to ion nitriding treatment and/or ion etching treatment in a cavity of coating equipment, selecting a Cr target, setting a target current to be 40-100A, applying negative bias of-20 to-50V on the substrate, controlling the heating temperature to be 400-450 ℃, keeping the argon flow at 300-350 sccm, and depositing for 0.5-1 h, so as to deposit and form the Cr layer on the surface of the substrate;
placing the substrate with the Cr layer deposited on the surface in a cavity of coating equipment, selecting Cr and an AlSi target, wherein the content of Al and Si in the AlSi target is 9: 1-1: 1, the target current is set to be 40-100A, applying negative bias of-20 to-50V on the substrate, controlling the heating temperature to be 400-450 ℃, keeping the argon flow to be 0-100 sccm, keeping the nitrogen flow to be 500-700 sccm, and depositing for 2-4 h, so that a CrAlSiN coating is formed by deposition, and the composite coating is formed;
the wear-resistant corrosion-resistant Cr/CrAlSiN composite coating comprises a bonding layer and a wear-resistant corrosion-resistant layer which are sequentially formed on a base body, wherein the bonding layer is a Cr layer, the wear-resistant corrosion-resistant layer is a CrAlSiN layer, the thickness of the composite coating is 5-20 micrometers, the thickness of the Cr layer is 0.2-1 micrometer, the thickness of the CrAlSiN layer is 4.8-19 micrometers, the CrAlSiN layer has an amorphous nanocrystalline structure and comprises a face-centered cubic CrN phase, an AlN reinforcing phase and an amorphous Si phase3N4Phase of the amorphous Si3N4The CrN phase and the AlN strengthening phase are wrapped, the content of the CrN phase in the CrAlSiN layer is 10-20 wt%, the content of the AlN phase is 6-10 wt%, and Si is contained in the CrAlSiN layer3N4The phase content is 15 to 45 wt%.
2. The method of claim 1, wherein: the Si content of the CrAlSiN layer is 2at.% to 10 at.%.
3. The production method according to claim 1, characterized by comprising: and cleaning the surface of the substrate, and then sequentially performing ion nitriding treatment and ion etching treatment on the clean substrate surface.
4. The production method according to claim 3, characterized in that: the surface cleaning treatment comprises: and sequentially carrying out ultrasonic cleaning on the surface of the matrix by using an oil removal agent and more than one organic solvent until the surface of the matrix is clean.
5. The method of claim 1, wherein: the substrate is a metal substrate.
6. The method of claim 5, wherein: the metal matrix comprises cemented carbide.
7. The method of claim 5, wherein: the metal matrix comprises stainless steel.
8. The method of claim 1, wherein: the purity of the high-purity argon is more than 99%.
9. The method of claim 1, wherein: the purity of the Cr target and the purity of the AlSi target are both more than 99.9 percent.
10. The method of claim 1, wherein: the purity of the nitrogen is more than 99.9 percent.
11. The method of claim 1, wherein: the coating equipment is internally provided with a plurality of groups of targets, each group of targets comprises more than one Cr target and more than one AlSi target, and one Cr target in each group of targets and one corresponding AlSi target are arranged in a mutually perpendicular mode.
12. The method of claim 1, further comprising: sequentially performing ion nitriding treatment and ion etching treatment on the surface of a substrate in a cavity of coating equipment, sequentially depositing a Cr layer and a CrAlSiN layer on the surface of the substrate, cooling the obtained composite coating to below 220 ℃ in a vacuum environment, and cooling to below 100 ℃ in a protective atmosphere.
13. Use of a wear and corrosion resistant Cr/craalsin composite coating prepared by the method according to any one of claims 1 to 12 in the field of surface protection of metallic and/or non-metallic materials.
14. Use according to claim 13, characterized in that: the metallic material and/or the non-metallic material comprise ocean engineering materials.
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| CN109930106B (en) * | 2019-05-08 | 2020-10-13 | 哈尔滨工业大学 | Preparation method of TiAlSi/TiAlSiN multilayer alternating coating with high wear resistance |
| CN110484889B (en) * | 2019-09-24 | 2021-06-22 | 中国科学院宁波材料技术与工程研究所 | Multilayer protective coating with high-temperature steam oxidation resistance and hot water corrosion resistance, and preparation method and application thereof |
| CN113322434B (en) * | 2021-06-04 | 2022-04-19 | 中国科学院宁波材料技术与工程研究所 | Nano composite coating and preparation method and application thereof |
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